Fifth Fusarium-toxin forum – 11 janvier 2008 Sampling program 2005-2007 Caroline DESGRANGES (ONIGC)
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Fifth Fusarium-toxin forum – 11 janvier 2008
Sampling program2005-2007
Caroline DESGRANGES (ONIGC)
Study co-ordinated & undertaken by :
IRTAC, ONIGC and ARVALIS-Institut du végétal
Fifth Fusarium-toxin forum – 11 janvier 2008
Financed by :
ONIGC, ANMAC, ARVALIS-Institut du végétal,Coop de France, FNA, SYNACOMEX, SNIA,
USIPA, GNIS
Regulation 401-2006 : 100 increments / 500 tonnes
Evaluate the accuracy using less than
100 increments / 500 t.
Problem posed
Fifth Fusarium-toxin forum – 11 janvier 2008
Norm EN ISO 24333
Available Data
Wheat : Sampling by vacuum spear during storage
Maize : Sampling in flowing grain at exit of silo
Mass of each increment : 750 à 2700g of grain
Fifth Fusarium-toxin forum – 11 janvier 2008
Regulation EC Sept 07 -Maximum levels in foods-
(ppb)
Mean values of studied silos
(ppb)Wheat 1 250 477 to 1 988Maize 1 750 2 633
DON
Fumonisines B1+B2 Maize 4 000 534 to 7 132
Zearalenone Maize 350 139 to 683
Fifth Fusarium-toxin forum – 11 janvier 2008
Available Data
1 582 mycotoxin analysis
Quantification of fumonisines B1+B2 by HPLC fluorometry with solidphase extraction clean up - NF EN ISO 13585
Quantification of zearalenone by HPLC fluorometry and immunoaffinty column clean up – normative project EN ISO 17372
Quantification of deoxynivalenol by HPLC UV and immunoaffintycolumn clean up – normative project EN ISO DON CEN/TC275/WG5/M383
0
1000
2000
3000
4000
5000
6000
1 6 11 16 21 26 31 36 41 46 51 56 61 66 71 76 81 86 91 96
N° Increments
DO
N p
pbDistribution within silos
-DON-
Silo 05-01
Fifth Fusarium-toxin forum – 11 janvier 2008
0
2000
4000
6000
8000
10000
12000
14000
16000
13579
111315171921232527293133353739414345474951535557596163656769717375777981838587899193959799
101103105107109111113115117119121123125127129131133135137139141143145147149
N° Increm
ents
B1+B2 ppb
Distribution
withinsilos
-Fumonisines-
Silo 07-01
Fifth Fusarium-toxin
forum –
11 janvier 2008
Statistical Analysis
µ̂
Fifth Fusarium-toxin forum – 11 janvier 2008
Estimation of the silo
mean
Error due to samplingTotal Error = + Error due to analysis
Silo Sample
Error due to sampling
TOTAL ERROR
Analysis
Error due to analysis
(several increments)
The coefficient of variation (CV) is independant from the mean
Fifth Fusarium-toxin forum – 11 janvier 2008
Statistical Analysis
0
10
20
30
40
50
60
70
0 1000 2000 3000 4000 5000 6000 7000 8000
Mean
CV
sam
plin
g
CV = 45%
3 working hypothesis
CV = 10%, 20% et 30%
Fifth Fusarium-toxin forum – 11 janvier 2008
Statistical analysis
Sampling error
Analytical error
Conclusions
Fifth Fusarium-toxin forum – 11 janvier 2008
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
0 10 20 30 40 50 60 70 80 90 100 110
Number of increments in 500 tonnes
Unc
erta
inty
on
estim
atio
n (%
)
CV analytical = 10% CV analytical = 20% CV analytical = 30%
Conclusions
• Overall accuracy of the result cannot be lower than analytical accuracy given by CVanalytical
• From a given number of increment samples the gain in precision becomes insignificant :
=> 100 increments + CVanalytical of 20% : uncertainty at +/- 41%
=> 25 increments + CVanalytical of 20% : uncertainty at +/- 44%
=> 10 increments + CVanalytical of 20% : uncertainty at +/- 50%
Fifth Fusarium-toxin forum – 11 janvier 2008
- 3 points
- 6 points
Conclusions
• Total Error = Sampling Error + Analytical Error
Fifth Fusarium-toxin forum – 11 janvier 2008
•This model is validated by an empirical approach
(simulation of the composition of 10 000 samples using 5, 10, 15… increments)
•This model is valid for :
DON, Fumonisines, Zearalenone
Wheat and Maize
Large panel of contaminations
Application :Decision aiding table
Fifth Fusarium-toxin forum – 11 janvier 2008
Number of increments
5 41 42 43 43 44 45 46 47 48 49 50 51 53 54 55 57 58 60 61 63 64 66 67 69 71 72
10 30 31 32 33 34 35 36 37 39 40 41 43 44 46 47 49 51 52 54 56 58 59 61 63 65 66
15 25 26 27 28 29 31 32 33 35 36 38 40 41 43 45 46 48 50 52 53 55 57 59 61 62 64
20 22 23 25 26 27 28 30 31 33 34 36 38 40 41 43 45 47 48 50 52 54 56 58 60 61 63
25 21 22 23 24 25 27 28 30 32 33 35 37 38 40 42 44 46 48 49 51 53 55 57 59 61 63
50 16 17 19 20 22 24 25 27 29 31 33 34 36 38 40 42 44 46 48 50 52 54 55 57 59 61
100 13 15 17 18 20 22 24 26 28 29 31 33 35 37 39 41 43 45 47 49 51 53 55 57 59 61
Infinity 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52 54 56 58 60
56 58 6048 50 52 5440 42 44 4632 34 36 3824 26 28 3016 18 20 22
Relative analytical uncertainty (%) 10 12 14
International normalization
Fifth Fusarium-toxin forum – 11 janvier 2008
• 2 norms in preparation :
European & international norm : EN ISO 24333
reviewing between march to october 2008 ; publication in 2009
Technical report (supporting norm EN ISO 24333), gatheringFrench, UK and German sampling studies : project EN ISO 29263
reviewing between may to july 2008 ; publication end of 2008
Fifth Fusarium-toxin forum – 11 janvier 2008
Sampling program2005-2007
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